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Absorption
Spectrometry
Analytical Methods
Notices Safety Notices
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NOTE When solvent extractions of perchloric acid solution are performed, some of the
acid may dissolve in the organic solvent that is subsequently aspirated. In addition,
if the organic solution is aspirated whilst floating on the surface of the acid, do not
allow the capillary tube to drop below the organic solvent and suck up aqueous
perchloric acid.
Clean the burner frequently — never allow the burner to clog, and wash it
thoroughly both inside and out.
Minimize the amount of acetone which is carried over with the acetylene by:
‘Cracking’ the bottle before use by gently opening the valve to check for any
drops or spray of acetone. Any bottle showing acetone should be returned to
the supplier for replacement.
Storing and using the bottles in the vertical position.
Using only one instrument per bottle.
Using only ‘instrument’ grade acetylene.
Replacing bottles when the pressure drops to 750 kPa (100 psi).
Ensure that all safety covers are in position, and wear approved ear protectors
and safety glasses.
Ensure the pressure relief bung of the spray chamber can be easily removed by
hand. Refit the bung according to the operation manual.
Contents
1. Introduction 9 Li (Lithium) 44
Ag (Silver) 15 Mg (Magnesium) 46
Al (Aluminium) 16 Mn (Manganese) 47
As (Arsenic) 18 Mo (Molybdenum) 48
Au (Gold) 19 Na (Sodium) 49
B (Boron) 20 Nb (Niobium) 50
Ba (Barium) 21 Nd (Neodymium) 51
Be (Beryllium) 22 Ni (Nickel) 52
Bi (Bismuth) 23 Os (Osmium) 53
Ca (Calcium) 24 P (Phosphorus) 54
Cd (Cadmium) 25 Pb (Lead) 55
Co (Cobalt) 26 Pd (Palladium) 56
Cr (Chromium) 27 Pr (Praseodymium) 57
Cs (Cesium) 28 Pt (Platinum) 58
Cu (Copper) 29 Rb (Rubidium) 59
Dy (Dysprosium) 30 Re (Rhenium) 60
Er (Erbium) 31 Rh (Rhodium) 61
Eu (Europium) 32 Ru (Ruthenium) 62
Fe (Iron) 33 Sb (Antimony) 63
Ga (Gallium) 34 Sc (Scandium) 64
Gd (Gadolinium) 35 Se (Selenium) 65
Ge (Germanium) 36 Si (Silicon) 66
Hf (Hafnium) 37 Sm (Samarium) 67
Hg (Mercury) 38 Sn (Tin) 68
Ho (Holmium) 39 Sr (Strontium) 69
In (Indium) 40 Ta (Tantalum) 70
Ir (Iridium) 41 Tb (Terbium) 71
K (Potassium) 42 Te (Tellurium) 72
La (Lanthanum) 43 Ti (Titanium) 73
1. Introduction
General 9
Safety Aspects 9
Reagents and Apparatus 10
Sample Preparation 10
Standard Preparation 10
Matrix Effects 11
Chemical Interferences 11
Nebulizers 13
Organic Solvents13
Recommended Instrument Parameters 14
General References 14
The sample to be analyzed can be brought Detailed methods for solvent extraction of
into solution by a number of means: metals can be found in the literature.
At low concentrations (less than 10 µg/mL) Physical Properties of Standard and Sample
solutions have been found to deteriorate quite
quickly because of adsorption on the walls of For a given flow of support gas, the amount of
the container. sample aspirated by the nebulizer and the
proportion which reaches the flame are
Similarly, standard addition solutions can be dependent on the physical properties of the
prepared containing all of the required solution — viscosity, surface tension, density,
elements. This will avoid multiple splitting of solvent vapor pressure. To avoid differences
the sample for individual elements and in the amount of sample and standard which
reduce the amount of time spent in preparing reach the flame, it is necessary that the
standards. physical properties of sample and standard
Before weighing, standard materials should be matched as closely as possible. If this
be treated to ensure that they are in a cannot be done, the method of standard
standard state. additions must be employed.
Oxides Ionization
It will be noted that in region B, small Where the interference assumes serious
variations in interferent level will cause large proportions, it is sometimes possible to
changes in the absorbance of the analyte extract the analyte element into an organic
element. Because this is analytically medium. When choosing a chelating agent it is
undesirable, the analyst should use a sample unnecessary to ensure high selectivity; it is
treatment procedure which will avoid only necessary to insure that the interferent
operating in region B. and analyte are separated. For example,
potassium interference on tantalum can be
Where interference is encountered, the avoided by extracting tantalum as the fluoride
following procedure for optimization of the complex into methyl isobutyl ketone, thus
flame stoichiometry is recommended: preventing the formation of refractory
1 Prepare two calibration standards having potassium fluorotantalate.
the same analyte element concentration Extract the Interferent
— one being prepared in distilled water
and the other in a synthetic matrix It is often possible to remove the interferent
corresponding to the sample material. by organically extracting if from solution. A
2 Light the flame and measure the highly specific and quantitative extraction is
absorbance of both solutions. Adjust the not always necessary. For example, in the
burner position for maximum determination of trace metals in iron ores, the
absorbance with the synthetic matrix excess iron can be extracted into isobutyl
solution, and adjust the fuel flow until acetate as the chloride complex. This allows
the absorbance of both solutions is trace analysis to be carried out on the
identical, or as close as possible. aqueous solution free of bulk iron.
General References
1. Dean, John A. and Rains, Theodore C.,
‘Flame Emission and Atomic Absorption
Spectroscopy’, Volume 1 — Theory, Volume
2 — Components and Techniques, Marcel
Dekker.
2. Mavrodineanu, R. and Boiteux, H., ‘Flame
Spectroscopy’, John Wiley and Sons.
3. Angino, E.F. and Billings, G.K., ‘Atomic
Absorption Spectrometry in Geology’,
Elsevier.
2. Standard Conditions
Flame Emission
Ag (Silver)
Wavelength 328.1 nm
A.W. 107.9
Slit width 0.1 nm
Preparation of Standard Solutions Fuel acetylene
Atomic Absorption
Working Conditions (Fixed)
Lamp current 4 mA
Fuel acetylene
Support air
Flame stoichiometry oxidizing
Working Conditions (Variable)
References
1. Marks, J.Y.and Welcher, G.G., Anal. Chem.,
42, (9), 1033 (1970).
2. Ramakrishna, T.V., et al., Anal. Chim.
Acta., 39, 81 (1967).
3. Ferris, A.P., et al., Analyst, 95, 574 (1970).
As (Arsenic) Interferences
A.W. 74.92 Spectral Interference
Flame stoichiometry reducing; red cone 5. Brodie, K.G., Amer. Lab., 11, 58 (1979).
1–2 cm high 6. Agilent Instruments At Work, No. AA-38.
Working Conditions (Variable)
Flame Emission
Arsenic is not generally determined by flame
emission because of the poor emission
characteristics of the element.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 4 mA
Fuel acetylene
Support air
Flame stoichiometry oxidizing
Working Conditions (Variable)
Flame Emission
Wavelength 267.6 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Interferences
Few interferences have been noted in air-
acetylene flames. However, large excesses of
iron, copper and calcium have been found to
suppress the result(1) where gold is extracted
into MIBK.
Solvent extraction techniques have been
developed(2), which remove any interfering
element.
B (Boron) Interferences
A.W. 10.81 Sodium has been found to cause interference
when the ratio of sodium to boron is very
high. The effect is usually minimized by
Preparation of Standard Solutions
adjusting the flame to neutral stoichiometry
(red cone 0.5–1 cm high) with consequent loss
Recommended Standard Materials of sensitivity.
Sodium Borate A.R. Grade Na2B4O7.10H2O
Boric Acid A.R. Grade H3BO3
Solution Technique
Dissolve 44.095 g of Na2B4O7.10.H2O in
500 mL water and dilute to
1 litre to give 5000 μg/mL B.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 20 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
(Note 1) 2–2.5 cm high
Note 1: Carefully adjust flame stoichiometry
and burner position for optimum sensitivity.
Working Conditions (Variable)
249.7
0.2 5–2000
249.8
208.9 0.2 15–4000
Flame Emission
Wavelength 249.7 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Generally a flame having a red cone 1 cm high
with at the burner 1–2 mm below the light
path will be found to be nearly optimum.
Boron is not usually determined by flame
emission because of the poor emission
characteristics of the element.
Ba (Barium) Interferences
A.W. 137.3 Barium is partially ionized in the nitrous
oxide-acetylene flame. To suppress ionization,
add potassium nitrate or chloride solution to
Preparation of Standard Solutions
give final concentration of 2000 μg/mL
potassium in all solutions including the blank.
Recommended Standard Materials The strong emission from barium falling on
Barium Carbonate A.R. Grade BaCO3 the photomultiplier may result in a
considerable increase in shot noise evidenced
Barium Chloride A.R. Grade BaCl2.2H2O by increasingly noisy signals as the
concentration of barium increases.
Solution Technique
Barium absorbance in an air-acetylene flame
Dissolve 1.7785 g of BaCl2.2H2O in water and is severely depressed by phosphate, silicon
dilute to 1 litre to give 1000 μg/mL Ba. and aluminium. This is overcome by the use
of a nitrous oxide-acetylene flame.
Recommended Instrument Parameters
Atomic Absorption
Working Conditions (Fixed)
Lamp current 20 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
2–3 cm high
Working Conditions (Variable)
Flame Emission
Wavelength 553.6 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Severe spectral interference will be observed
when measuring barium in the presence of
calcium due to a strong CaOH band occurring
around the same wavelength.
Be (Beryllium) References
A.W. 9.012 1. Ramakrishna, T.V., West, P.W. and
Robinson, J.W., Anal. Chim. Acta., 39, 81–
87 (1967).
Preparation of Standard Solutions
2. Fleet, B., Liberty, K.V. and West, T.S.,
Recommended Standard Materials Talanta, 17, 203–210 (1970).
Beryllium metal strip or wire 99.99%
Beryllium oxide 99.99%
Solution Technique
Dissolve 1.000 g of beryllium metal in 20 mL
of 1:1 sulfuric acid containing a trace of
hydrochloric acid. Dilute to 1 litre to give
1000 μg/mL Be.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 5 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
1–2 cm
Working Conditions (Variable)
Wavelength (nm) 234.9
Slit width (nm) 1.0
Optimum working range (μg/mL) 0.01–4
Flame Emission
Wavelength 234.9 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Interferences
Sodium and silicon at levels in excess of
1000 μg/mL have been found to severely
depress beryllium absorbance.
Aluminium has been reported (1,2) to
suppress the absorbance by 25%. This was
overcome by the presence of 1.5 g/L of
fluoride.
Bi (Bismuth) Interferences
A.W. 209.00 No chemical interference at levels up to
10000 μg/mL interferent has been reported
for the determination of bismuth with an air-
Preparation of Standard Solutions
acetylene flame.
Flame Emission
Wavelength 223.1 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
The use of flame emission for bismuth is not
recommended because of the poor emission
characteristics of the element.
Ca (Calcium) Interferences
A.W. 40.08 Chemical interferences in the air-acetylene
flame are pronounced and have been fairly
well documented(1,2,3,4). These interferences,
Preparation of Standard Solutions
which depress the calcium absorbance, can be
eliminated by the introduction of a releasing
Recommended Standard Materials agent such as strontium (5000 μg/mL) or
Calcium carbonate CaCO3 lanthanum (10000 μg/mL). Normally the
addition of a releasing agent is used in
Solution Technique conjunction with the practice of matching
sample and standard solutions to obviate
Dissolve 2.497 g of dried calcium carbonate in combined interference effects.
a minimum volume of 1:4 nitric acid. Dilute to
1 litre to give 1000 μg/mL Ca. The presence of excess sodium or potassium
causes 5–10% signal enhancement due to
suppression of ionization.
Recommended Instrument Parameters
In the nitrous oxide-acetylene flame the main
Atomic Absorption interference is caused by ionization of
calcium itself. This is overcome by the
Working Conditions (Fixed) addition of a more readily ionisable element
Lamp current 10 mA such as potassium (2000–5000 μg/mL).
Flame Emission
Wavelength 422.7 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Maximum intensity is obtained with an
oxidizing nitrous oxide-acetylene flame (red
cone 1 mm high).
Cd (Cadmium) Interferences
A.W. 112.4 No major chemical interference has been
reported in the air-acetylene flame.
Preparation of Standard Solutions
Solution Technique
Dissolve 1.000 g of cadmium in a minimum
volume of 1:1 nitric acid. Dilute to 1 litre to
give 1000 μg/mL Cd.
Atomic Absorption
Working Conditions (Fixed)
Lamp current (Note 1) 4 mA
Fuel (Note 2) acetylene
Support air
Flame stoichiometry oxidizing
Note 1: Absorbance strongly dependent on
lamp current.
Note 2: Absorbance strongly dependent on
flame stoichiometry. Adjust the fuel flow
carefully for maximum sensitivity.
Working Conditions (Variable)
Flame Emission
Wavelength 326.1 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Cadmium is not usually determined by flame
emission because of the poor emission
characteristics of the element.
Solution Technique
Dissolve 1.000 g of metal in a minimum
volume of 1:1 nitric acid and dilute to 1 litre
to give 1000 μg/mL Co.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 7 mA
Fuel acetylene
Support air
Flame stoichiometry oxidizing
Working Conditions (Variable)
Flame Emission
Wavelength 345.4 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Interferences
Few interferences have been observed for
cobalt in an air-acetylene flame.
It has been reported that nickel levels in
excess of 1500 μg/mL cause severe depression
of about 50%.
Fuel acetylene
Support air
Flame stoichiometry reducing
Working Conditions (Variable)
Flame Emission
Wavelength 425.4 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Interferences
Cobalt, iron and nickel (particularly in the
presence of perchloric acid) have been found
to cause depression of chromium absorbance.
Cs (Cesium)
A.W. 132.9
Solution Technique
Dissolve 1.2667 g of dried CsCl in water and
dilute to 1 litre to give 1000 μg/mL Cs.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 20 mA
Fuel acetylene
Support air
Flame stoichiometry oxidizing
Working Conditions (Variable)
Flame Emission
Wavelength 852.1 nm
Slit width 0.1 nm
Fuel acetylene
Support air
To remove the possibility of second order
spectral interference, it is recommended that
a filter be used to cut off wavelengths below
600 nm.
Interferences
No interference from normal matrix elements
has been reported.
Cu (Copper) Interferences
A.W. 63.54 No interferences have been reported for
copper in the air-acetylene flame, but some
depression has been noted at high Zn/Cu
Preparation of Standard Solutions
ratios. This can be minimized by the use of a
lean air-acetylene flame or a nitrous oxide-
Recommended Standard Materials acetylene flame.
Copper metal strip or wire 99.99%
Solution Technique
Dissolve 1.000 g of copper metal in a
minimum volume of 1:1 nitric acid and dilute
to 1 litre to give 1000 μg/mL Cu.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 4 mA
Fuel acetylene
Support air
Flame stoichiometry oxidizing
Working Conditions (Variable)
Flame Emission
Wavelength 327.4 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Dy (Dysprosium) Interferences
A.W. 162.5 Hydrofluoric acid, aluminium and silicon
have been found to depress the absorbance by
90%. The interference is increased by the
Preparation of Standard Solutions
presence of sodium.
Flame Emission
Wavelength 526.5 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Below 10 μg/mL, determination by flame
emission is preferred, although the
wavelength required must be accurately
isolated to avoid spectral interference from
the other rare earth elements. At higher
concentrations, atomic absorption is normally
used.
Er (Erbium) Interferences
A.W. 167.3 As in the case of other rare earth elements,
severe interference is observed in the
presence of hydrofluoric acid, aluminium and
Preparation of Standard Solutions
silicon, particularly when measured in the
presence of sodium.
Recommended Standard Materials
Erbium is partially ionized in the nitrous
Erbium oxide Er2O3 99.9% oxide-acetylene flame. To suppress ionization,
add potassium nitrate or chloride solution to
Solution Technique give a final concentration of 4000 μg/mL
Dissolve 1.1400 g of erbium oxide in 1:1 potassium in all solutions including the blank.
hydrochloric acid and dilute to 1 litre to give
1000 μg/mL Er. References
1. Kinnunen, J. and Lindsjo, O., Chemist-
Recommended Instrument Parameters Analyst, 56, 76–78 (1967).
Atomic Absorption
Working Conditions (Fixed)
Lamp current 10 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
1–2 cm high
Working Conditions (Variable)
Flame Emission
Wavelength 400.8 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Below 10 μg/mL, determination by flame
emission is preferred, although the
wavelength required must be accurately
isolated to avoid spectral interference from
other rare earth elements. At higher
concentrations, atomic absorption is normally
used.
Eu (Europium) Interferences
A.W. 152.0 As in the case of other rare earth elements,
severe interference is observed in the
presence of hydrofluoric acid, silicon and
Preparation of Standard Solutions
aluminium when measured in the presence of
sodium.
Recommended Standard Materials
Interference may be minimized by the
Europium oxide Eu2O3 99.9% precipitation of the rare earth oxide and
subsequent dissolution in hydrochloric acid.
Solution Technique
Europium is partially ionized in the nitrous
Dissolve 1.1579 g of Eu2O3 in a minimum oxide-acetylene flame. To suppress ionization,
volume of 1:1 hydrochloric acid and dilute add potassium nitrate or chloride solution to
quantitatively to 1 litre with water to give give a final concentration of 4000 µg/mL
1000 μg/mL Eu. potassium in all solutions including the blank.
Flame Emission
Wavelength 459.4 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Below 10 µg/mL, determination by flame
emission is preferred, although the
wavelength required must be accurately
isolated to avoid spectral interference from
other rare earth elements. At higher
concentrations, atomic absorption is normally
used.
Flame Emission
Wavelength 372.0 nm
Slit width 0.1 nm
Fuel acetylene
Support air
Interferences
Interference from citric acid has been
reported(1) to suppress the absorbance by up
to 50% for a citric acid level of 200 μg/mL. The
effect is not overcome by adjustment of flame
stoichiometry.
Ga (Gallium) Interferences
A.W. 69.72 Interferences have not been reported for
atomic absorption measurements using the
air-acetylene flame. Any interferences may be
Preparation of Standard Solutions
readily overcome by using the nitrous oxide-
acetylene flame with little loss in sensitivity.
Recommended Standard Materials Gallium is partially ionized in the nitrous
Gallium metal 99.9% oxide-acetylene flame. To suppress ionization,
add potassium nitrate or chloride solution to
Solution Technique give a final concentration of 2000 μg/mL
potassium in all solutions including the blank.
Dissolve 1.000 g of gallium metal in a
minimum volume of 1:1 nitric acid and dilute For emission measurements, manganese
to 1 litre to give 1000 μg/mL Ga. causes spectral interference by emitting at
403.3 nm. This can be overcome by using the
417.2 nm line and establishing the baseline by
Recommended Instrument Parameters scanning.
Atomic Absorption
Working Conditions (Fixed)
Lamp current (Note 1) 4 mA
Fuel acetylene
Support air
Flame stoichiometry oxidizing
Note 1: Absorbance is highly dependent on
lamp current.
Working Conditions (Variable)
Flame Emission
Wavelength 403.3 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Gd (Gadolinium) Interferences
A.W. 157.25 Gadolinium is partially ionized in the nitrous
oxide-acetylene flame. To suppress ionization,
add potassium nitrate or chloride solution to
Preparation of Standard Solutions
give a final concentration of 2000 μg/mL
potassium in all solutions including the blank.
Recommended Standard Materials
Hydrofluoric acid, iron, aluminium and
Gadolinium oxide Gd2O3 99.9% silicon each severely depress gadolinium
absorbance when present at concentrations in
Solution Technique excess of 500 μg/mL.
Dissolve 1.1526 g of Gd2O3 in a minimum
volume of 1:1 hydrochloric acid and dilute to
1 litre to give 1000 μg/mL Gd.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 20 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
1–2 cm high
Working Conditions (Variable)
Flame Emission
Wavelength 461.7 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Below 500 μg/mL, determination by flame
emission is preferred, although the
wavelength required must be accurately
isolated to avoid spectral interference from
the other rare earth elements. At higher
concentrations, atomic absorption is normally
used.
Atomic Absorption
Working Conditions (Fixed)
Lamp current (Note 1) 5 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
(Note 2) 1–2 cm high
Note 1: Absorbance is slightly dependent on
lamp current.
Hf (Hafnium) Interferences
A.W. 178.5 Hafnium absorbance has been found to be
suppressed by sulfuric acid, hydrofluoric
acid, alkali metals and alkaline earth metals.
Preparation of Standard Solutions
Most transition group metals interfere. In
many cases the interferents affect the
Recommended Standard Materials absorbance when present in concentrations
Hafnium metal 99.9% as small as 50 μg/mL, with hafnium at
100 μg/mL. The use of an oxidizing nitrous
Solution Technique oxide-acetylene flame can minimize most of
these effects. However, the development of
Dissolve 1.000 g of hafnium metal strip in analytical techniques where the interferent is
5 mL hydrofluoric acid, 5 mL water by the usually present at minimal concentrations is
slow DROPWISE addition of 10 mL of recommended. Matrices of sample and
concentrated nitric acid. Allow the reaction to standard solutions must be carefully matched.
subside before each addition. Dilute to 1 litre
to give 1000 μg/mL Hf.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 10 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
1–2 cm high
Working Conditions (Variable)
Flame Emission
Wavelength 368.2 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Hafnium is usually determined by atomic
absorption.
Hg (Mercury) Interferences
A.W. 200.59 Mercury (I) and mercury (II) show different
sensitivities in the air-acetylene flame.
Preparation of Standard Solutions Mercury (I) is more sensitive due to the
disproportionation reaction.
Recommended Standard Materials
Hg22+ →Hg2+ + Hg0
Mercury metal 99.99%
Elemental mercury is readily atomized with
Mercuric Chloride A.R. Grade HgCl2 100% efficiency.
The ‘cold vapor technique’ can be used for
Solution Technique trace determinations of mercury(1,5). Metallic
Dissolve 1.354 g of mercuric chloride in ions which are reduced to the elemental state
10 mL nitric acid. Dilute to 1 litre to give by stannous chloride can interfere with the
1000 μg/mL Hg. cold vapor method. They can amalgamate or
form stable compounds with mercury(2,3).
Recommended Instrument Parameters With both flame and cold vapor techniques, it
is advisable to check for the absence of non-
Atomic Absorption atomic absorption.
Working Conditions (Fixed)
References
Lamp current 4 mA
1. Poluektov, N.S., and Vitkun, R.A., Zhur.
Fuel acetylene Anal. Chim., 18, (1), 37 (1963).
Support air 2. Poluektov, N.S., Vitkun, R.A. and Zelukova,
Y.V., ibid., 19, (8), 937 (1964).
Flame stoichiometry oxidizing
3. Brodie, K.G., Amer. Lab., 9, 73 (1977).
Working Conditions (Variable)
4. Brodie, K.G., Amer. Lab., 11, 58 (1979).
Wavelength (nm) 253.7
5. Agilent Instruments At Work, No. AA-38.
Slit width (nm) 0.5
Optimum working range (μg/mL) 2–400
Flame Emission
Wavelength 253.7 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Mercury is not usually determined by flame
emission.
Ho (Holmium) Interferences
A.W. 164.9 Holmium is partially ionized in the nitrous
oxide-acetylene flame. To suppress ionization,
add potassium nitrate or chloride solution to
Preparation of Standard Solutions
give a final concentration of 2000 μg/mL
potassium in all solutions including the blank.
Recommended Standard Materials Holmium absorbance has been found to be
Holmium oxide Ho2O3 99.9% suppressed by hydrofluoric acid, aluminium
and silicon.
Solution Technique
Dissolve 1.146 g of holmium oxide in a
minimum volume of 1:1 hydrochloric acid.
Dilute to 1 litre to give 1000 μg/mL Ho.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 20 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
1–2 cm high
Working Conditions (Variable)
Flame Emission
Wavelength 559.0 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Below 25 μg/mL, determination by flame
emission is preferred, although the
wavelength required must be accurately
isolated to avoid spectral interference from
the other rare earth elements. At higher
concentrations, atomic absorption is normally
used.
Solution Technique
Dissolve 1.000 g of indium metal in a
minimum volume of 1:1 nitric acid and dilute
to 1 litre to give 1000 μg/mL In.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 5 mA
Fuel (Note 1) acetylene
Support air
Flame stoichiometry oxidizing
Note 1: Fuel flow must be adjusted carefully
for optimum sensitivity and detection limit
conditions.
Working Conditions (Variable)
Flame Emission
Wavelength 451.1 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Flame stoichiometry oxidizing: red cone
0.5 cm high
Interferences
Indium is substantially ionized in the nitrous
oxide-acetylene flame. To suppress ionization,
add potassium nitrate or chloride solution to
give a final concentration of 2000 μg/mL
potassium in all solutions including the blank.
Ir (Iridium) Interferences
A.W. 192.2 Chemical interference in the air-acetylene
flame is extremely diverse(1). In simple
solutions, the overall effect of a particular
Preparation of Standard Solutions
element is markedly dependent on the
concentration ratio of iridium to interferent.
Recommended Standard Materials In general, aluminium, copper, lead,
Ammonium chloroiridate A.R. (NH4)2IrCl6 platinum, sodium and potassium enhance the
absorbance by over 50%; titanium, tin, nickel,
Iridium powder 99.9% iron and palladium tend to depress the signal
by amounts greater than 30%. The
Solution Technique interference pattern in the complex matrix of
ores, minerals etc. is extremely difficult to
Dissolve 2.294 g of (NH4)2IrCl6 in a minimum
categorize.
volume of 10% hydrochloric acid. Dilute to
1 litre to give 1000 μg/mL Ir. Fortunately, an empirical means of
overcoming the major interference effects has
Recommended Instrument Parameters been reported(2). Although (in common with
many releasing agents) the chemistry of the
Atomic Absorption reaction has not been investigated, it has been
found that a copper-sodium mixture
Working Conditions (Fixed) (7000 μg/mL Cu; 3000 μg/mL Na) is very
effective in counteracting the interferences.
Lamp current 20 mA
The mixture is prepared from the sulfate salts
Fuel (Note 1) acetylene of the respective elements. Copper nitrate, at
a much higher level (20000 μg/mL Cu) has
Support air also been used to overcome these
Flame stoichiometry reducing; interferences(3).
slightly luminous
References
Note 1: Absorbance is highly dependent on
the flame stoichiometry and the acetylene 1. Van Loon, J.C., Atomic Abs. Newsletter, 8,
flow rate must be carefully optimized. (1), 6 (1969).
Working Conditions (Variable) 2. Grimaldi, F.S. and Schnepfe, M.M.,
Talanta, 17, 617, (1970).
Wavelength Slit Width Optimum Working
(nm) (nm) Range (µg/L) 3. Houze, A.A.G., Journal South African
Chem. Inst., 23, 115, (1970).
208.9 0.2 5–200
264.0 0.2 12–480
266.5 0.2 15–560
254.4 0.2 20–720
Flame Emission
Wavelength 380.0 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Iridium is usually determined by atomic
absorption.
K (Potassium) Interferences
A.W. 39.10 Potassium is partially ionized in the air-
acetylene flame. To suppress ionization, add
cesium nitrate or chloride solution to give a
Preparation of Standard Solutions
final concentration of 1000 μg/mL cesium in
all solutions including the blank. The purest
Recommended Standard Materials available cesium compound must be used to
Potassium chloride KCl A.R. Grade avoid potassium contamination.
Solution Technique
Dissolve 1.907 g of dried potassium chloride
in water and dilute to 1 litre to give
1000 μg/mL K.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 5 mA
Fuel (Note 1) acetylene
Support air
Flame stoichiometry oxidizing
Note 1: An air-acetylene flame is normally
used because interferences are reduced and
the signal/noise ratio is improved.
Working Conditions (Variable)
Flame Emission
Wavelength 766.5 nm
Slit width 0.1 nm
Fuel acetylene
Support air
The flame emission determination of
potassium is limited by flame stability and by
‘pick up’ of potassium from the air and
storage vessels. Air-acetylene can be used if
an ionization suppressant is added.
La (Lanthanum) Interferences
A.W. 138.9 Lanthanum is partially ionized in the nitrous
oxide-acetylene flame. To suppress ionization,
add potassium nitrate or chloride solution to
Preparation of Standard Solutions
give a final concentration of 5000 μg/mL
potassium in all solutions including the blank.
Recommended Standard Materials
Both absorption and emission signals for
Lanthanum oxide La2O3 99.99% lanthanum are depressed in the presence of
phosphates, fluorides, silicon, aluminium and
Solution Technique iron, and by other rare earths. Many solvent
Dissolve 11.730 g of La2O3 in a minimum extraction procedures can be found in the
volume of 1:1 nitric acid and dilute to 1 litre literature; one simple method is extraction at
to give 10000 μg/mL La. pH 7 with 0.1 M cinnamic acid in hexane.
Otherwise rigorous matching of sample and
standard solutions is necessary to control
Recommended Instrument Parameters interferences. No chemical releasing agent
has been discovered.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 20 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
1.5–2 cm
Working Conditions (Variable)
Flame Emission
Wavelength 441.7 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
The flame emission signal for lanthanum is
quite intense. Determination by flame
emission is therefore preferred, although the
wavelength required must be accurately
isolated to avoid spectral interference from
the other rare earth elements.
Li (Lithium) Interferences
A.W. 6.939 In the air-acetylene flame, ionization is
appreciable and it is necessary to match all
solutions with respect to easily ionized
Preparation of Standard Solutions
elements such as Na, K, Rb, Cs, Ca, Sr and Ba.
Ionization is suppressed if all solutions are
Recommended Standard Materials made to contain 2000 μg/mL potassium. No
Lithium carbonate Li2CO3 99.9% chemical interferences are known.
Solution Technique
Dissolve 5.324 g of Li2CO3 in a minimum
volume of 1:5 nitric acid and dilute to 1 litre
to give 1000 μg/mL Li.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 5 mA
Fuel acetylene
Support air
Flame stoichiometry oxidizing
Working Conditions (Variable)
Flame Emission
Wavelength 670.8 nm
Slit width 0.1 nm
Fuel acetylene
Support air
Flame Emission
Wavelength 466.2 nm or 451.9 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Note that the emission at 466.2 nm arises
from the LuO band emission, while at
451.9 nm the emission is a line due to Lu
atoms.
Magnesium metal strip or wire 99.99% The nitrous oxide-acetylene flame shows no
interference except a general absorbance
Solution Technique enhancement of 15% by the alkali metals due
to suppression of ionization.
Dissolve 1.000 g of magnesium in 1:4 nitric
acid. Dilute to 1 litre to give 1000 μg/mL Mg.
References
Recommended Instrument Parameters 1. Halls, D.J. and Townshend, A., Anal.
Chim. Acta., 38, 278 (1966).
Atomic Absorption 2. Firman, R.J., Spectrochim. Acta., 21, 341
Working Conditions (Fixed) (1965).
Flame Emission
Wavelength 285.2 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Interferences
The most common interferences in air-
acetylene can be overcome by the addition of
a known excess of a releasing agent such as
strontium (1000–5000 μg/mL) or lanthanum
(10000 μg/mL). Solutions containing
200 μg/mL interferent in 0.4 μg/mL Mg show
the following interference pattern:
Mn (Manganese) Interferences
A.W. 54.94 In a reducing air-acetylene flame the
absorbance is depressed in the presence of
phosphate, perchlorate, iron, nickel, silicon
Preparation of Standard Solutions
and cobalt. In an oxidizing air-acetylene flame
or a nitrous oxide-acetylene flame these
Recommended Standard Materials interferences do not arise. No releasing agent
Manganese metal strip or wire 99.99% is usually necessary.
Solution Technique
Dissolve 1.000 g manganese in a minimum
volume of 1:1 nitric acid and dilute to 1 litre
to give 1000 μg/mL Mn.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 5 mA
Fuel acetylene
Support air
Flame stoichiometry oxidizing
A nitrous oxide-acetylene flame can also be
used but sensitivity is poorer.
Working Conditions (Variable)
Flame Emission
Wavelength 403.1 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Mo (Molybdenum) Interferences
A.W. 95.94 Conflicting statements have been made on
interferences in molybdenum atomic
absorption. Various workers have found
Preparation of Standard Solutions
either no interferences or severe
interferences from all metals, apparently
Recommended Standard Materials depending on the solution conditions. In the
Molybdenum metal strip or wire 99.99% recommended nitrous oxide-acetylene flame
interferences can be suppressed by adding an
Solution Technique excess of a refractory element (1000 μg/mL
Al).
Dissolve 1.000 g molybdenum in hot
concentrated nitric acid, cool, and dilute to References
1 litre to give 1000 μg/mL Mo.
1. David, D.J., Analyst, 86, 730 (1961).
Recommended Instrument Parameters 2. Ramakrishna, T.V., West, P.W. and
Robinson, J.W., Anal. Chim. Acta., 44, 437,
Atomic Absorption (1969).
Working Conditions (Fixed) 3. Kirkbright, G.D., Smith, A.M. and West,
T.S., Analyst, 91, 700 (1966).
Lamp current 7 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry strongly reducing;
red cone 2–3 cm.
A brightly luminous air-acetylene flame can
be used with poorer sensitivity and increased
interference effects.
Working Conditions (Variable)
Flame Emission
Wavelength 390.3 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Na (Sodium)
A.W. 22.99
Solution Technique
Dissolve 2.542 g of dried NaCl in water and
dilute to 1 litre to give 1000 μg/mL Na.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 5 mA
Fuel acetylene
Support air
Flame stoichiometry oxidizing
Working Conditions (Variable)
330.2
0.5 2–400
330.3
Flame Emission
Wavelength 589.0 nm
Slit width 0.1 nm
Fuel acetylene
Support air
Interferences
Sodium is partially ionized in the air-
acetylene flame. To suppress ionization, add
potassium nitrate or chloride solution to give
a final concentration of 2000 μg/mL
potassium in all solutions including the blank.
Nb (Niobium) Interferences
A.W. 92.91 Hydrofluoric acid increases the absorbance
signal up to 2% HF, but greater concentrations
depress the signal. Sodium in the presence of
Preparation of Standard Solutions
2% HF depresses the signal. By analogy with
zirconium it is expected that 0.1 M NH4F
Recommended Standard Materials would eliminate some of these interferences
Niobium metal 99.99% and enhance the signal, although data for Nb
has not been published.
Solution Technique Niobium is appreciably ionized in the nitrous
Dissolve 5.000 g of niobium metal strip in oxide-acetylene flame and it is therefore
5 mL hydrofluoric acid, 5mL water by the recommended to add about 0.1% potassium
slow DROPWISE addition of 10 mL of chloride as an ionization suppressant.
concentrated nitric acid. Dilute to 1 litre to
give 5000 μg/mL Nb. References
1. Thomas, P.E. and Pickering, W.F., Talanta,
Recommended Instrument Parameters 18, 127 (1971).
Flame Emission
Wavelength 405.9 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Nd (Neodymium) Interferences
A.W. 144.2 Neodymium is partially ionized in the nitrous
oxide-acetylene flame. To suppress ionization,
add potassium nitrate or chloride solution to
Preparation of Standard Solutions
give a final concentration of 2000 μg/mL
potassium in all solutions including the blank.
Recommended Standard Materials The signal is depressed in the presence of
Neodymium oxide Nd2O3 99.99% 500 μg/mL silicon, aluminium, iron, titanium
or fluoride. A more oxidizing flame reduces
Solution Technique these effects.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 20 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
1–2 cm
Working Conditions (Variable)
Flame Emission
Wavelength 660.8 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
The flame emission signal for neodymium is
quite intense. Below 350 μg/mL,
determination by flame emission is preferred,
although the wavelength required must be
accurately isolated to avoid spectral
interference from the other rare earth
elements. At higher concentrations, atomic
absorption is normally used.
Solution Technique
Dissolve 1.340 g OsO4 in 100 mL water with
the addition of a sodium hydroxide pellet to
assist dissolution. Dilute to 1 litre to give
1000 μg/mL Os.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 20 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
1–2 cm
An air-acetylene flame can also be used but
with poorer sensitivity.
Working Conditions (Variable)
P (Phosphorus) References
A.W. 30.97 1. Hobbins, William B., "Direct Determination
of Phosphorus in Aqueous Matrices by
Atomic Absorption", Agilent Instruments
Preparation of Standard Solutions
At Work, Number AA-19 (1982).
Solution Technique
Dissolve 37.138 g of dried NH4H2PO4 in water.
Dilute to 1 litre to give 10000 μg/mL P.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 10 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
1–2 cm
Working Conditions (Variable)
Wavelength (nm) 213.6
Slit width (nm) 1.0
Optimum working range (μg/mL) 400–30000
Flame Emission
This method is not recommended.
Interferences
The relative lack of sensitivity of phosphorus
means that determination by flame atomic
absorption spectrometry is not common and
the literature contains few references. It is
recommended that either an interference
study be carried out or matrix-matched
standards be used.
Pb (Lead) Interferences
A.W.207.19 No cationic interferences have been reported
for the air-acetylene flame, however a number
of anionic interferences have been reported.
Preparation of Standard Solutions
Phosphate, carbonate, iodide, fluoride and
acetate suppress lead absorbance
Recommended Standard Materials significantly at concentrations ten times
Lead metal strip or wire 99.9% greater than lead. These interferences can be
largely overcome by addition of EDTA
Solution Technique solution so that the sample solutions are
0.1 molar with respect to EDTA.
Dissolve 1.000 g of lead in 1:1 nitric acid.
Dilute to 1 litre to give 1000 μg/mL Pb. At the 217.0 nm wavelength, non-atomic
species in the flame absorb strongly. Where
the sample has a high concentration of
Recommended Instrument Parameters dissolved solids it is necessary to correct for
non-atomic absorption.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 5 mA
Fuel acetylene
Support air
Flame stoichiometry oxidizing
Working Conditions (Variable)
Flame Emission
Wavelength 405.8 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Pd (Palladium) Interferences
A.W. 106.4 In the air-acetylene flame the atomic
absorption signal is depressed in the presence
of aluminium, cobalt or nickel at all
Preparation of Standard Solutions
concentrations and by hydrofluoric acid. The
depression is eliminated in the presence of
Recommended Standard Materials lanthanum (5000 μg/mL as chloride) or EDTA
Ammonium chloropalladite (NH4)2PdCl4 99.9% (0.01 M). The interference can be reduced by
using a more oxidizing flame and by taking
Solution Technique measurements higher in the flame. A nitrous
oxide-acetylene flame can be used to
Dissolve 2.672 g of ammonium chloropalladite overcome the interferences, but the
in water and dilute to 1 litre to give sensitivity is much poorer.
1000 μg/mL Pd.
References
Recommended Instrument Parameters
1. Sychra, V., Slevin, P.J., Matousek, J. and
Bek, F., Anal. Chim. Acta., 52, 259 (1970).
Atomic Absorption
Working Conditions (Fixed)
Lamp current 5 mA
Fuel acetylene
Support air
Flame stoichiometry oxidizing
Working Conditions (Variable)
Flame Emission
Wavelength 363.5 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Pr (Praseodymium) Interferences
A.W. 140.9 Praseodymium is partially ionized in the
nitrous oxide-acetylene flame. To suppress
ionization, add potassium nitrate or chloride
Preparation of Standard Solutions
solution to give a final concentration of
2000 μg/mL potassium in all solutions
Recommended Standard Materials including the blank.
Praseodymium oxide Pr2O3 99.9% The atomic absorption signal is depressed in
the presence of silicon at high concentrations
Solution Technique (>2000 μg/mL).
Dissolve 1.170 g of Pr2O3 in 5 mL hydrochloric
acid and dilute to 100 mL to give
10000 μg/mL Pr.
Atomic Absorption
Working Conditions (Fixed)
Lamp current (Note 1) 10 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
1–2 cm
Note 1: Absorbance is much lower at
increased lamp current.
Working Conditions (Variable)
Flame Emission
Wavelength 284.0 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
The flame emission signal for praseodymium
is quite intense. Below 800 μg/mL,
determination by flame emission is preferred,
although the wavelength required must be
accurately isolated to avoid spectral
interference from the other rare earth
elements. At higher concentrations, atomic
absorption is normally used.
Pt (Platinum) References
A.W. 195.09 1. Schnepfe, M.M., and Grimaldi, F.S.,
Talanta, 16, 591 (1969).
Preparation of Standard Solutions 2. Strasheim, A. and Wessels, G.J., Appl.
Spectrosc., 17, 65 (1963).
Recommended Standard Materials
3. Pitts, A.G., Van Loon, J.C. and Beamish,
Ammonium chloroplatinate (NH4)2PtCl6 99.9% F.E., Anal. Chim. Acta., 50, 181 (1970); 50,
195 (1970).
Solution Technique
Dissolve 2.275 g of (NH4)2PtCl6 in water and
dilute to 1 litre to give 1000 μg/mL Pt.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 10 mA
Fuel acetylene
Support air
Flame stoichiometry oxidizing
Working Conditions (Variable)
Flame Emission
Wavelength 266.0 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Interferences
The atomic absorption signal is depressed in
the presence of most other noble metals, and
also in the presence of acids. The
interferences can be reduced (but not
eliminated) by using a more oxidizing flame.
Interferences are eliminated if all solutions
are made 2% in copper or 1% in lanthanum.
A nitrous oxide-acetylene flame can be used
to overcome the interferences but the
sensitivity is poorer.
Solution Technique
Dissolve 1.415 g of dried RbCl in water and
dilute to 1 litre to give 1000 μg/mL Rb.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 20 mA
Fuel acetylene
Support air
Flame stoichiometry oxidizing
Working Conditions (Variable)
Flame Emission
Wavelength 780.0 nm
Slit width 0.1 nm
Fuel acetylene
Support air
Interferences
Rubidium is 40–50% ionized in the air-
acetylene flame. To suppress ionization, add
potassium nitrate or chloride solution to give
a final concentration of 2000 μg/mL
potassium in all solutions including the blank.
Re (Rhenium)
A.W. 186.2
Solution Technique
Dissolve 1.554 g of KReO4 in water and dilute
to 1 litre to give 1000 μg/mL Re.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 20 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
1–2 cm
Working Conditions (Variable)
Flame Emission
Wavelength 346.1 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Interferences
The atomic absorption signal for rhenium is
enhanced in the presence of sulfuric acid
(0.1%–5%) and depressed in the presence of
calcium, barium or magnesium (>100 μg/mL).
Most transition group metals depress the
signal slightly at any concentration. All of
these interferences can be minimized by using
a slightly more oxidizing flame.
Flame Emission
Wavelength 369.2 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Interferences
In an air-acetylene flame, most other elements
interfere and the interference depends
unpredictably on their concentration.
Phosphoric and sulfuric acids depress the
signal (constant above 10% concentration).
Alkali metal sulfates, on the other hand,
enhance the signal strongly although other
sulfates give mixed results.
Flame Emission
Wavelength 372.8 nm
Slit width 0.1 nm
Fuel acetylene
Support air
Interferences
In an air-acetylene flame most other elements
and most acids interfere in an unpredictable
manner. The only releasing agent discovered
so far is uranyl nitrate (4% w/v U), which
overcomes all interferences except the
depression due to Ti(III).
Sb (Antimony) Interferences
A.W. 121.75 In an air-acetylene flame, copper and nickel
depress the signal, especially in a reducing
flame. A more oxidizing flame removes the
Preparation of Standard Solutions
effect.
Note1: The nitrous oxide-acetylene flame 4. Brodie, K.G., Amer. Lab., 11, 58 (1979).
may also be used but shows reduced 5. Agilent Instruments At Work, No. AA-38.
sensitivity.
Working Conditions (Variable)
Flame Emission
Wavelength 259.8 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Flame Emission
Wavelength 402.0 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Interferences
Scandium is partially ionized in the nitrous
oxide-acetylene flame. To suppress ionization,
add potassium nitrate or chloride solution to
give a final concentration of 2000 μg/mL
potassium in all solutions including the blank.
Se (Selenium) References
A.W. 78.96 1. Nakahara, T. et al., Anal. Chim. Acta., 50,
51 (1970).
Preparation of Standard Solutions 2. Brodie, K.G., Amer. Lab., 9, 73 (1977).
3. Brodie, K.G., Amer. Lab., 11, 58 (1979).
Recommended Standard Materials
4. Agilent Instruments At Work, No. AA-38.
Selenium metal pellets 99.9%
Solution Technique
Dissolve 1.000 g of selenium metal in 80 mL
of 1:1 nitric acid, heat gently to initiate the
reaction — cool if the reaction proceeds too
vigorously. Cool and dilute to 1 litre to give
1000 μg/mL Se.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 10 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry highly reducing
Working Conditions (Variable)
Flame Emission
Selenium is not generally determined by
flame emission because of the poor emission
characteristics of the element.
Interferences
At 196.0 nm and 204.0 nm, non-atomic
species in the flame absorb strongly. Use a
background corrector.
Si (Silicon) Interferences
A.W. 28.09 Severe depression of silicon absorbance has
been observed in the presence of hydrofluoric
acid, boric acid and potassium at significant
Preparation of Standard Solutions
levels (1%).
Solution Technique
Fuse 2.14 g of silicon dioxide with 8 g of
sodium hydroxide in a zirconium crucible at
dull red heat until a clear melt is obtained.
Cool, dissolve the cake in 100 mL of 1:3
hydrochloric acid and make up to 1 litre to
give 1000 μg/mL Si.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 10 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry strongly reducing;
yellow outer edge;
red cone 2–3 cm high
Working Conditions (Variable)
Flame Emission
Wavelength 251.6 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Sm (Samarium) Interferences
A.W. 150.4 Samarium is partially ionized in the nitrous
oxide-acetylene flame. To suppress ionization,
add potassium nitrate or chloride solution to
Preparation of Standard Solutions
give a final concentration of 2000 μg/mL
potassium in all solutions including the blank.
Recommended Standard Materials
Samarium oxide Sm2O3 99.9%
Solution Technique
Dissolve 1.159 g of Sm2O3 in 10 mL 1:1
hydrochloric acid and dilute to 1 litre to give
1000 μg/mL Sm.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 10 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
1–1.5 cm
Working Conditions (Variable)
Flame Emission
Wavelength 442.4 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
The flame emission signal for samarium is
quite intense. Below 300 μg/mL,
determination by flame emission is preferred,
although the wavelength required must be
accurately isolated to avoid spectral
interference from the other rare earth
elements. At higher concentrations, atomic
absorption is normally used.
Solution Technique
Dissolve 1.000 g of tin in 100 mL hydrochloric
acid (warm to 60°C if necessary). Cool and
dilute to 1 litre to give 1000 μg/mL Sn in 1:9
hydrochloric acid. All further dilutions are
made with 1:9 hydrochloric acid or 1%
tartaric acid.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 7 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
2 cm
Working Conditions (Variable)
Flame Emission
Wavelength 284.0 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Interferences
The nitrous oxide-acetylene flame is
recommended for all tin determinations.
Sr (Strontium) Interferences
A.W. 87.62 In the air-acetylene flame, silicon, aluminium,
titanium, zirconium, phosphate and sulfate
depress the signal at all concentrations. These
Preparation of Standard Solutions
effects can be removed by adding 1%
lanthanum as nitrate or chloride to all
Recommended Standard Materials solutions, or 0.01 M EDTA with 2000 μg/mL
Strontium carbonate SrCO3 99.99% lanthanum.
In the nitrous oxide-acetylene flame these
Solution Technique interferences do not occur.
Dissolve 1.685 g SrCO3 in 10 mL 1:1 nitric Strontium is partially ionized in all flames. To
acid and dilute to 1 litre to give 1000 μg/mL suppress ionization, add potassium nitrate or
Sr. chloride solution to give a final concentration
of 2000 μg/mL potassium in all solutions
Recommended Instrument Parameters including the blank.
Flame Emission
Wavelength 460.7 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Ta (Tantalum) Interferences
A.W. 180.95 Fluoride and ammonium ions in the absence
of alkali metals increase the absorbance
signal. In the presence of alkali metals and
Preparation of Standard Solutions
fluoride the absorbance is depressed. Sulfate
depresses the absorbance, and phosphate
Recommended Standard Materials enhances it up to 2% phosphoric acid — higher
Tantalum metal 99.9% concentrations of phosphate depress the
absorbance.
Solution Technique In the absence of alkali metals, the addition of
Dissolve 1.000 g of tantalum metal strip in ammonium fluoride to all solutions (0.1 M)
10 mL hydrofluoric acid, 5 mL water by the gives improved sensitivity and reduces acid
slow DROPWISE addition of 10 mL of interferences. In the presence of alkali metals
concentrated nitric acid. Allow the reaction to no releasing agents are known. Tantalum (V)
subside before each addition. Dilute to 1 litre cupferrate can be extracted from 0.5% tartrate
to give 1000 μg/mL Ta. systems at pH 0 with isoamyl alcohol.
Tantalum as the fluoride is extracted from
6 M sulfuric acid, 10 M hydrofluoric acid +
Recommended Instrument Parameters 2.2 M ammonium fluoride medium into
methyl isobutyl ketone.
Atomic Absorption
It has been found that the addition of
Working Conditions (Fixed) 2000 μg/mL of aluminium improves the
Lamp current 20 mA linearity of tantalum determination(5).
Flame Emission
Wavelength 481.3 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Solution Technique
Dissolve 5.881 g of Tb4O7 in 20 mL of 1:1
hydrochloric acid and dilute to 1 litre to give
5000 μg/mL Tb.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 20 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
1–1.5 cm
Working Conditions (Variable)
Flame Emission
Wavelength 596.6 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Interferences
Terbium is partially ionized in the nitrous
oxide-acetylene flame. To suppress ionization,
add potassium nitrate or chloride solution to
give a final concentration of 2000 μg/mL
potassium in all solutions including the blank.
Flame Emission
Wavelength 214.3 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
The determination of tellurium by flame
emission is not recommended.
Interferences
No severe interferences have been
encountered in the air-acetylene flame.
Ti (Titanium) Interferences
A.W. 47.90 Most metallic elements enhance the titanium
absorbance signal at concentrations above
500 μg/mL, probably by competing with
Preparation of Standard Solutions
titanium for the available oxygen in the flame
and reducing the refractory titanium oxide.
Recommended Standard Materials Sodium above 1000 μg/mL depresses the
Titanium metal 99.99% signal; fluoride, chloride, and ammonium ions
enhance it. Releasing agents include:
Solution Technique 1000 μg/mL Al in HCl
Dissolve 1.000 g of titanium metal strip in 2000 μg/mL KCl
10 mL of hydrofluoric acid, 10 mL water by
the slow, DROPWISE addition of 20 mL nitric 0.1 M NH4F
acid. Allow the reaction to subside before
each addition. Dilute to 1 litre to give References
1000 μg/mL Ti.
1. Thomas, P.E. and Pickering, W.F., Talanta,
18, 127 (1971).
Recommended Instrument Parameters
2. Willis, J.B., Appl. Opt., 7, 1295 (1968).
Atomic Absorption 3. Bond, A.M., Anal. Chem., 42, 932 (1970).
Working Conditions (Fixed)
4. Mostyn, R.A. and Cunningham, A.F., At.
Lamp current 20 mA Abs. Newsl, 6, 86 (1967).
Flame Emission
Wavelength 399.8 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Solution Technique
Dissolve 1.303 g of dried TlNO3 in 20 mL 1%
nitric acid and dilute to 1 litre to give
1000 μg/mL Tl.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 10 mA
Fuel acetylene
Support air
Flame stoichiometry oxidizing
Working Conditions (Variable)
Flame Emission
Wavelength 535.1 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Interferences
No interferences have been reported in an air-
acetylene flame.
Thallium is partially ionized in the nitrous
oxide-acetylene flame.
To suppress ionization, add potassium nitrate
or chloride solution to give a final
concentration of 2000 μg/mL potassium in all
solutions including the blank.
Tm (Thulium) Interferences
A.W. 168.9 Thulium is partially ionized in the nitrous
oxide-acetylene flame. To suppress ionization,
add potassium nitrate or chloride solution to
Preparation of Standard Solutions
give a final concentration of 2000 μg/mL
potassium in all solutions including the blank.
Recommended Standard Materials
Thulium oxide Tm2O3 99.9%
Solution Technique
Dissolve 1.142 g of Tm2O3 in 20 mL 1:1
hydrochloric acid and dilute to 1 litre to give
1000 μg/mL Tm.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 20 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
1–2 cm
Working Conditions (Variable)
Flame Emission
Wavelength 410.6 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
The flame emission signal for thulium is quite
intense. Below 10 μg/mL, determination by
flame emission is preferred, although the
wavelength required must be accurately
isolated to avoid spectral interference from
the other rare earth elements. At higher
concentrations, atomic absorption is normally
used.
U (Uranium) Interferences
A.W. 238.0 Uranium is partially ionized in the nitrous
oxide-acetylene flame. To suppress ionization,
add potassium nitrate or chloride solution to
Preparation of Standard Solutions
give a final concentration of 4000 μg/mL
potassium in all solutions including the blank.
Recommended Standard Materials
Uranyl nitrate, UO2(NO3)2.6H2O A.R. Grade
Solution Technique
Dissolve 21.10 g of uranyl nitrate in water
and dilute to 1 litre to give 10000 mg/mL U.
This should be treated as a hazardous
chemical, and normal precautions for
handling radioactive materials must be
observed.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 20 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
1–1.5 cm
Working Conditions (Variable)
Flame Emission
Wavelength 591.5 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
V (Vanadium) References
A.W. 50.94 1. Sachdev, S.L., Robinson, J.W. and West,
P.W., Anal. Chim. Acta., 37, 12 (1967).
Preparation of Standard Solutions 2. Bond, A.M., Anal. Chem., 42, 932 (1970).
3. Thomas, P.E. and Pickering, W.F., Talanta,
Recommended Standard Materials
18, 127 (1971).
Vanadium metal granules 99.99%
Solution Technique
Dissolve 1.000 g of vanadium in 40 mL nitric
acid and dilute to 1 litre to give 1000 μg/mL V.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 20 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
1–1.5 cm
Working Conditions (Variable)
Flame Emission
Wavelength 437.9 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Interferences
Vanadium is not as greatly affected as
niobium or tantalum by alkali metal fluorides.
Ammonium (0.1 M NH4F) enhances the signal,
as do a large range of other species. The
interferences are removed by adding
aluminium (2:1 excess or 2000 μg/mL).
Atomic Absorption
Working Conditions (Fixed)
Lamp current 20 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
1–2 cm
Working Conditions (Variable)
Flame Emission
Wavelength 400.9 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Detection limit 3 μg/mL
Interferences
The 400.9 nm resonance line may be
preferred because of an improved signal-to-
noise ratio.
Solution Technique
Dissolve 1.270 g Y2O3 in 20 mL hydrochloric
acid and dilute to 1 litre to give 1000 μg/mL Y.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 10 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
1.5–2 cm
Working Conditions (Variable)
Flame Emission
Wavelength 407.7 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Interferences
The absorbance signal is depressed in the
presence of aluminium, potassium and
phosphoric acid at all concentrations.
Yb (Ytterbium) Interferences
A.W. 173.04 Ytterbium is partially ionized in the nitrous
oxide-acetylene flame. To suppress ionization,
add potassium nitrate or chloride solution to
Preparation of Standard Solutions
give a final concentration of 2000 μg/mL
potassium in all solutions including the blank.
Recommended Standard Materials
Ytterbium absorbance and emission signals
Ytterbium oxide Yb2O3 99.9% are depressed in the presence of hydrofluoric
acid, iron, aluminium and silicon at all
Solution Technique concentrations.
Dissolve 1.139 g of Yb2O3 in 20 mL
hydrochloric acid and dilute to
1 litre to give 1000 μg/mL Yb.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 5 mA
Fuel acetylene
Support nitrous oxide
Flame stoichiometry reducing; red cone
1.5–2 cm
Working Conditions (Variable)
Flame Emission
Wavelength 398.8 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
The flame emission signal for ytterbium is
quite intense. Below 3 μg/mL, determination
by flame emission is preferred, although the
wavelength required must be accurately
isolated to avoid spectral interference from
the other rare earth elements. At higher
concentrations, atomic absorption is normally
used.
Zn (Zinc) Interferences
A.W. 65.37 No chemical interferences have been found in
an air-acetylene flame. When working with
biological samples, ashing is necessary to
Preparation of Standard Solutions
avoid the physical effects of protein
molecules on nebulizer performance. At the
Recommended Standard Materials 213.9 nm wavelength, non-atomic species in
Zinc metal granules 99.99% the flame absorb strongly. Where the sample
has a high concentration of dissolved solids it
Solution Technique is necessary to correct for non-atomic
absorption.
Dissolve 1.000 g of zinc in 40 mL 1:1
hydrochloric acid and dilute to
1 litre to give 1000 μg/mL Zn.
Atomic Absorption
Working Conditions (Fixed)
Lamp current 5 mA
Fuel acetylene
Support air
Flame stoichiometry oxidizing
All other conventional flames can be used.
Working Conditions (Variable)
Flame Emission
Wavelength 213.9 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Flame Emission
Wavelength 360.1 nm
Slit width 0.1 nm
Fuel acetylene
Support nitrous oxide
Interferences
Zirconium is ionized in this flame and 0.1%
potassium (as chloride) should be added to
suppress ionization.
It is best to avoid oxygen containing anions
(sulfate, nitrate) which tend to suppress the
absorbance.
References
1. Reichel, W. and Acs, L., Anal. Chem., 41,
(13), 1886 (1969).
2. Truscott, E.D., ibid, 42, (13), 1657 (1970).
Method 1 Analysis
Take replicate absorbance readings of the
Range sample and standard solutions. Compare
0.5–5.0 mg Cl these absorbances and calculate the
concentration of excess silver in the sample
Interferences solution.
Excess silver (mg/L) = mg/L Ag x dilution factor
Iodide, bromide, cyanide and sulfide interfere
by precipitating as silver compounds. Therefore:
Chromate interference is minimized under
the dilute acid conditions specified. Amount of = [100 - concentration of excess silver
chloride in (mg/L)] x 0.329 x sample solution
Reagents sample volume (mL) / 1000
solution
Silver solution: Refer to silver standard (mg)
conditions above. Prepare a solution
containing 1000 mg/L Ag. Concentration = amount of chloride (mg) /
of chloride volume of sample aliquot (litre)
Nitric acid: Extra pure, chloride-free (S.G. (mg/L)
1.40).
Method 2
Sample Preparation
Place an aliquot of sample solution, Range
containing 0.5 to 5.0 mg of chloride, in a 0.5–5.0 mg chloride
200 mL volumetric flask. Add 20 mL of
1000 mg/L silver solution and 1 mL chloride-
Interferences
free nitric acid. Make up to volume with
distilled water. The solution contains Bromide and cyanide interfere by
100 mg/L Ag. precipitation silver compounds which are
soluble in ammonia. Iodide and chromate
Allow the mixture to stand overnight in a
interference is minimized under the
dark place to prevent photochemical
conditions specified.
reactions taking place. Centrifuge an aliquot
of the supernatant liquid slurry for
10 minutes. For analysis, take 10 mL of the Reagents
clear solution and dilute to 100 mL with Silver solution: Refer to silver standard
distilled water. For a sample containing conditions above.
5.0 mg chloride, the analytical solution will Prepare a solution
contain approximately 9.3 mg/L excess silver. containing 1000 mg/L Ag.
Standard Preparation
Refer to silver standard conditions above.
Prepare a standard containing 50 mg/L Ag in
1% (v/v) chloride-free nitric acid.
Prepare calibration standards containing 0,
1.0, 2.5, 5.0, 7.5, 10.0 mg/L Ag.
Instrument Parameters
Refer to silver standard conditions above.
Use the 338.3 nm wavelength.
Analysis
Take replicate absorbance readings of the
sample and standard solutions. Compare the
absorbances and calculate the concentration
of silver in solution and hence the
concentration of chloride in the sample.
Concentration of = mg/L Ag x dilution factor
silver (mg/L)
Amount of = concentration of silver found
chloride in (mg/L) x 0.329 x sample solution
sample volume (mL) / 1000
solutions
(mg)
Standard Preparation
Fuse 2.14 g of A.R. silicon dioxide with 8 g of
A.R. sodium hydroxide in a zirconium
crucible. Heat to a dull red heat until a clear
melt is obtained. Cool, dissolve the melt in
100 mL of 1:3 hydrochloric acid and make up
to 1 litre to give a solution containing
1000 mg/L silicon. Prepare a standard
containing 10 mg/L Si by dilution of the
1000 mg/L silicon solution.
Take 1, 3, 5, 10 mL aliquots of the 10 mg/L
silicon standard to give 0.01, 0.02, 0.05,
0.1 mg silicon. Treat the standard aliquots in
the same manner as the sample solution and
determine the molybdenum absorbance for
this range of silicon.
References Range
1. Cullum, D.C. and Thomas, D.B., Analyst, 0.2–2.0 mg SO4
85, 688 (1960).
2. Dunk, R., Mostyn, R.A. and Hoare, H.C., Reagents
Atomic Absorption News, 8, (4), 79 (1969). Barium solution (200 mg/L Ba): Refer to
barium standard conditions above. Prepare a
Barium Standard Conditions solution containing 200 mg/L Ba by dilution
of a 1000 mg/L barium standard.
Preparation of Standard Solutions Hydrochloric acid (0.2 M): Dilute 1.8 mL of
Recommended Standard Materials concentrated hydrochloric acid to 100 mL
with distilled water.
Barium carbonate BaCO3
Barium chloride BaCl2.2H2O
Solution Technique
Dissolve 1.7785 g of BaCl2.2H2O in water and
dilute to 1 litre to give 1000 μg/mL Ba.
Instrument Parameters
Refer to barium standard conditions above.
Use the 553.6 nm wavelength.
Analysis
Take replicate absorbance readings of the
barium in the sample and sulfate standard
solutions.
4. Methodology
Agriculture 93
Biochemical 98
Chemical 103
Food 108
Industrial 111
Mineral 121
Metallurgy 135
Petroleum 159
Pollution 161
Optimum Range
Agriculture
50–300 ng arsenic i.e., in this preparation
Laying Meal 0.005–0.30 μg/mL in solution or 5–30 μg/g in
the sample.
Mn (Manganese) Interferences
Typical Analysis At the 193.7 nm wavelength, non-atomic
Mn 0.01% absorption due to molecular species will
necessitate the use of background correction.
Sample Preparation
Chemical interferences can be encountered in
Wet-ash 2.5 g samples with nitric acid and the generation of arsine. Oxidizing agents can
perchloric acid. Dilute to 100 mL to give prevent the reaction entirely. Excess nitric
approximately 2.5 mg/mL Mn in solution. acid in particular must be absent from the
test solution.
Standard Preparation
Special Reagents
Prepare calibration standards containing 0,
2.5, 5, 10 mg/mL Mn, matching the sample in Ensure that all reagents are as free as
perchloric acid content. possible from arsenic.
Hydrochloric acid — Aristar Grade
Orchard Leaves (NBS Standard)
Sodium borohydride — Laboratory Grade
As (Arsenic) To prepare 5% solution, dissolve 5 g of sodium
Vapor Generation Technique borohydride in distilled water containing
0.1 g/100 mL of sodium hydroxide.
At low concentrations, this element can be
determined by the vapor generation
technique. Details of the appropriate
procedures are given in the operation manual
supplied with the Agilent vapor generation
accessory. Refer also to Agilent Instruments
At Work, No. AA-38.
Sample Preparation
Weigh 1.000 g of dried orchard leaves WARNING Explosion HazardOrganic
standard material and place in a clean perchlorates are explosive. Refer
crucible. Mix with 8 mL or 50% w/v to the warning message on Page 3
magnesium nitrate ashing aid. Place the of this book.
crucible on the hot plate and bring the
contents to boil. Allow to foam, but ensure
that no sample is lost. When the foaming Dissolve the residue in 2 mL nitric acid and
ceases, cover the crucible and transfer to a dilute to 50 mL with the addition of
muffle furnace set at 200°C. After two hours 2000 μg/mL potassium. For 150 μg/g Ca, the
raise the temperature to 500°C and ash for solution concentration will be approximately
about 8 hours. 3 μg/mL Ca.
Place 20 mL replicate aliquots into 50 mL Shake vigorously for one hour and filter
stoppered test tubes or phials. Using a pH through ammonium acetate washed Whatman
meter, adjust the pH of the solutions to 6–7 540 paper. Make up the volume to 100 mL
with 2.5 N sodium hydroxide and 2.5 N with distilled water (solution A for K). Dilute
sulfuric acid. Add 2 mL 1% (w/v) sodium 10 mL of prepared solution to 100 mL with
diethyldithiocarbamate, stopper the vessel distilled water. Add 500 μg/mL potassium
and shake for one minute to allow chelation (solution B for Ca/Mg).
to occur. Add 3 mL methyl isobutyl ketone
For sample with 300 μg/g Ca, the dilute
and shake in a rapid, even manner for
solution will contain 3 μg/mL Ca.
4–5 minutes. Allow the phases to separate
over 30 minutes. Use the clear, organic phase Standard Preparation
for analysis.
Refer to calcium standard conditions.
For 0.3 μg/g Tl, the organic portion will
contain approximately 0.3 μg/mL Tl. References
References Mn (Manganese)
1. Varju, M.E. and Elek, E., Atomic Range
Absorption Newsl., 10, 128 (1971).
0–200 μg/g Mn.
2. Varju, M.E., Agrokemia Talajtan, 19, 323
(1970). Interferences
3. Ure, A.M, Analytica Chimica Acta., 52, No chemical interferences experienced when
247 (1970). analyzing extracts containing up to
100 μg/mL Al, Ca, Fe, K, Mg, Na and P(2).
4. Dagnall, R.M., Kirkbright, R.M. and West,
T.S., Anal. Chem., 43, 1765 (1970). Sample Preparation
Refer to preparation of soil extract for
K (Potassium) copper. Use two-fold dilution of the extract
for determination. For a sample containing
Range
30 μg/g Mn, the concentration of diluted
0–80 μg/g solution will be 3 μg/mL Mn.
Sample Preparation Standard Preparation
Refer to procedure recommended for calcium Refer to manganese standard conditions.
in soil extract.
Prepare calibration solutions containing 0, 1,
Use original, undiluted solution; for 8 μg/g K, 2, 5 μg/mL Mn.
the solution will contain 0.8 μg/mL K.
The standards must be made up in 0.05 M
Standard Preparation EDTA and should contain major matrix
elements present in the sample solutions at
Make up calibration standards containing 0, approximately the same level.
0.2, 0.5, 1.0, 2.0 μg/mL K in 1 N ammonium
acetate. References
1. Ure, A.M. and Berrow, M.L., Analytica
Mg (Magnesium) Chimica Acta., 52, 247 (1970).
Range 2. Hossner, L.R. and Ferrara, L.W., Atomic
0–100 μg/g Absorption Newsl., 6, 71 (1967).
Interferences Zn (Zinc)
In the air-acetylene flame chemical Range
interferences are overcome by the addition of
a releasing agent such as strontium or 0.01–5.8 μg/g
lanthanum.
Sample Preparation
Analysis in the nitrous oxide-acetylene flame
Refer to preparation of soil extract for copper
is free from inter-element interference.
analysis. For 5.8 μg/g Zn in the sample,
Sample Preparation solution will contain 1.16 μg/mL Zn.
Refer to procedure recommended for calcium. Standard Preparation
Use dilute solution. For 20 μg/g Mg, the
Prepare standards containing 0, 0.5, 1.0,
solution will contain 0.2 μg/mL Mg.
2.0 μg/mL Zn. Use 0.05 M EDTA solution in
Standard Preparation dilution of the standards. Concentrations of
elements, other than zinc, present in the
Prepare calibration solutions containing 0, sample solution should be matched in the
0.1, 0.2, 0.5 μg/mL Mg in 1 N ammonium standards.
acetate.
Each solution should contain 5000 μg/mL
potassium.
Interferences
WARNING The nitrous oxide-acetylene flame is used to
Add the sodium hydroxide in overcome interferences from phosphates.
small increments of 1–3 mL, Calcium is partially ionized in this flame. To
cooling down between each suppress ionization, add potassium nitrate or
addition to control the violent chloride to give a final concentration of
reaction or else a serious injury 2000 μg/mL potassium in all solutions
could result. including the blank.
Sample Preparation
When most of the acid has been neutralized, Dilute 1 mL sample to 5 mL with distilled
as shown by a slowing down of the reaction, water. Centrifuge the solution for ten minutes
add a few drops of thymol blue indicator and to separate the protein matter. Decant the
continue the neutralization with the dropwise supernatant liquid into the original flask; use
addition of 50% (w/v) sodium hydroxide. this clear solution for all subsequent
Transfer to a 100 mL volumetric flask and operations.
make up to volume with distilled water.
Dilute 1 mL of the prepared solution to 25 mL
Place 20 mL replicate aliquots into 50 mL with distilled water with the addition of
stoppered test tubes or phials. Using a pH potassium to a concentration of 2000 μg/mL.
meter, adjust the pH of the solutions to 6–7 For 160 μg/mL Ca, the analytical solution will
with 2.5 N sodium hydroxide and 2.5 N contain approximately 1 μg/mL Ca at a
sulfuric acid. Add 2 mL 1% (w/v) sodium dilution of 1/125 the original sample.
diethyldithiocarbamate, stopper the vessel
and shake for one minute to allow chelation Standard Preparation
to occur. Add 3 mL methyl isobutyl ketone
Refer to calcium standard conditions.
and shake in a rapid, even manner for
4–5 minutes. Allow the phases to separate Prepare calibration standards containing 0,
over 30 minutes. Use the clear, organic phase 0.5, 1.0, 1.5 μg/mL Ca in 2000 μg/mL
for analysis. potassium.
For 0.3 μg/g Tl, the organic portion will
contain approximately 0.3 μg/mL Tl. Cu (Copper)
Typical Analysis
Standard Preparation
Refer to calcium in chicken blood plasma.
Refer to thallium standard conditions.
Sample Preparation
Prepare calibration standards containing 0,
0.5, 1, 5, 10, 20, 30 μg/mL Tl. Take 20 mL Refer to calcium in chicken blood plasma.
aliquots of the standard solution and adjust
the pH, chelate and extract with methyl Use the centrifuged solution; no further
isobutyl ketone as above (see sample dilution is required (dilution factor 1/5). For
preparation). 1.6 μg/mL Cu, the solution concentration will
be approximately 0.3 μg/mL Cu.
Chicken Plasma Standard Preparation
Refer to copper standard conditions.
Ca (Calcium)
Prepare calibration standards containing 0,
Typical Analysis
0.1, 0.2, 0.3, 0.4 μg/mL Cu.
Ca 160 μg/mL Mg 24 μg/mL
Mg (Magnesium)
Cu 1.6 μg/mL Zn 2.2 μg/mL
Typical Analysis
Refer to calcium in chicken blood plasma.
Sample Preparation
Refer to calcium in chicken blood plasma.
Use the 1/125 dilution solution. For 24 μg/mL
Mg, the solution concentration will be
approximately 0.2 μg/mL Mg.
Standard Preparation
Refer to magnesium standard conditions.
Prepare calibration standards containing 0,
0.1, 0.2, 0.3 μg/mL Mg with 2000 μg/mL
potassium added to match the sample
solution matrix.
Zn (Zinc)
Typical Analysis
Refer to calcium in chicken blood plasma.
Sample Preparation
Refer to calcium in chicken blood plasma.
Use the centrifuged solution; no further
dilution is required (dilution factor 1/5).
For 2.2 μg/mL Zn, the solution concentration
will be approximately 0.4 μg/mL Zn.
Standard Preparation
Refer to zinc standard conditions.
Prepare calibration standards containing 0,
0.3, 0.5, 1.0 μg/mL Zn.
Typical Analysis For 34.0% As, the dilute solution will contain
approximately 35 μg/mL As.
H2SO4 97.0% As 0.001%
Standard Preparation
Interferences
Refer to arsenic standard conditions.
At 193.7 nm, non-atomic species in the flame
absorb strongly. Use a background corrector Prepare calibration standards containing 0,
to check for the presence of background 20, 30, 40, 50 μg/mL As in 5% v/v ethanol.
absorption.
Si (Silicon)
Sample Preparation
Typical Analysis
Cautiously add 10 mL sulfuric acid sample to
15 mL water, using a pipette with filler bulb. Si 11.0%
Cool, dilute to 25 mL.
S, C and H remainder
Standard Preparation
Interferences
Refer to arsenic standard conditions.
The method of standard additions is used to
Prepare a 10 μg/mL As solution. compensate for the sample matrix.
For 15% Cd, the final solution concentration Dilute aliquots of this solution with xylene to
will be approximately 15 μg/mL Cd. give 50, 100, 150, 200, 300 μg/mL Sn
standards.
Standard Preparation
Dissolve 0.2084 g of cadmium Zn (Zinc)
cyclohexanebutyrate (24.0% Cd) in 2 mL Range
xylene and 4 mL 2-ethylhexylamine with
gentle heating. Cool and dilute to 100 mL with Suitable for hexanoic and octanoic acid salts
xylene to give a 500 μg/mL Cd stock solution. and other compounds soluble in xylene or
other organic solvents.
Dilute aliquots of this solution with xylene to
give standard solutions containing 0, 5, 10, Sample Preparation
20 μg/mL Cd.
Dissolve 0.500 g sample in xylene and dilute
with xylene to 100 mL. Dilute 1 mL to 100 mL
Pb (Lead) with xylene. For 10% Zn in a 0.500 g sample
Range this is 5 μg/mL Zn in solution.
10–20% Pb
Organic Complex
Co (Cobalt)
Typical Analysis
Co 10%
Food Na (Sodium)
Range
Beer
Up to 300 μg/mL Na
Fe (Iron) Typical Analysis
Typical Analysis Fe 0.1 μg/mL K 700 μg/mL Na 200 μg/mL
Fe 0.1 μg/mL Sample Preparation
Interferences Refer to iron in beer. Dilute 25 mL beer to
50 mL.
Interference is experienced from the
dissolved carbon dioxide causing irregular For 200 μg/mL Na, the solution concentration
aspiration of the sample. This is overcome by will be approximately 100 μg/mL Na.
degassing the sample prior to analysis. The
Standard Preparation
viscosity levels of some beers can cause
standardization problems and it is Refer to sodium standard conditions.
recommended that a standard addition
technique be used. Prepare standards containing 0, 50, 100,
150 μg/mL Na, with the addition of 350 μg/mL
Background correction is used to correct for K and an appropriate alcohol level to match
non-atomic absorption. the sample.
Sample Preparation
Fish
De-gas the sample by pouring it into a beaker
and stirring vigorously to ensure air
Hg (Mercury)
entrainment.
Cold vapor technique
Dilute duplicate 25 mL aliquots of sample to
50 mL, with the addition of 0.5 mL of a Interferences
10 μg/mL Fe solution to one of the aliquots.
Various materials in the fish digest interfere,
Standard Preparation and the method of standard additions must
therefore be used.
Refer to iron standard conditions.
At 253.7 nm, non-atomic species in the
Prepare a standard solution containing
sample may absorb strongly. Use a
10 μg/mL Fe.
background corrector to check for the
presence of background absorption.
K (Potassium)
Sample Preparation(1)
Typical Analysis
Weigh 5.0 g of ground sample into a 250 mL
K 400 μg/mL digestion flask equipped with a ground glass
Sample Preparation joint. Add 25 mL concentrated sulfuric acid,
20 mL 1:1 nitric acid,1 mL of 2% sodium
Partially de-gas the sample by pouring it into molybdate solution and boiling chips.
a beaker and stirring vigorously. Dilute 1 mL
sample to 500 mL. Connect a water-cooled condenser (packed
with 6 mm Raschig rings) to the digestion
For 400 μg/mL K, the solution concentration flask and reflux gently for 1 hour. Allow the
will be approximately 0.8 μg/mL K. flask to cool for 15 minutes then add 20 mL of
1:1 nitric acid/perchloric acid mixture
Standard Preparation
through the condenser.
Refer to potassium standard conditions.
Turn off the cooling water and boil the
Prepare calibration standards containing 0, mixture until white fumes appear in the flask.
0.5, 0.75, 1.0 μg/mL K. Continue heating for 10 minutes.
Gently heat duplicate 100 g lots of sample in Refer to manganese standard conditions.
silica dishes until the fatty acid self-ignites. Prepare calibration standards containing 0,
Allow to burn freely with no further 0.05, 0.1 μg/mL Mn. The standard solutions
application of heat. must contain the same reagents and major
Wet the carbonaceous residue with 2–3 mL matrix elements as the sample solutions at
sulfuric acid; heat to drive off excess acid and approximately the same concentration. For
ignite at 650–700°C. Dissolve the residue in example, in the typical case above the
10 mL 6 N hydrochloric acid, add 0.1 g standards would contain:
potassium as nitrate and dilute to 50 mL. K 2000 μg/mL
Prepare a reagent blank in the same manner.
HCl 1.2 N
For 0.1 μg/g Al, the solution concentration
will be approximately 0.2 μg/mL Al.
Industrial Cement
Interferences References
To overcome the inter-element interferences 1. Bernas, B., Anal. Chem., 40, 1682, (1968).
the nitrous oxide-acetylene flame was used.
2. ‘Methods for Analysis of NBS Clay
Addition of potassium (2000–5000 μg/mL)
prevents the loss of sensitivity due to Standards’, Special Publication 260-37,
ionization. June (1972).
Sn (Tin) Ca 10 μg/mL
Mineral Interferences
Sulfate ion depresses the calcium absorbance
Fluorspar by 30%. This effect is overcome readily in a
nitrous oxide-acetylene flame. Calcium is
Ba (Barium) partially ionized in this flame. To suppress
ionization, add potassium nitrate or chloride
Typical Analysis to give a final concentration of 2000 μg/mL
potassium in all solutions including the blank.
CaF2 98% Ba 0.04%
Sample Preparation
Interferences
Fluoride must be removed from the sample Dissolve 1.000 g sample in 20 mL of 1:1
hydrochloric acid.
during the fuming step to prevent
precipitation of insoluble barium fluoride. Cool and dilute to 100 mL.
Sample Preparation Dilute a 1 mL aliquot of the sample solution
Dissolve 0.500 g of fluorspar in 3 mL to 100 mL with the addition of 2000 μg/mL
hydrochloric acid and fume to dryness twice. potassium.
Cool, add 2 mL perchloric acid and heat to For 25% Ca, the final solution concentration
fumes. Cool, add 2 mL hydrofluoric acid and will be approximately 25 μg/mL Ca.
heat to fumes of perchloric acid appear.
Standard Preparation
Cool, dissolve in water and dilute to 100 mL
with the addition of 10 mL of 20000 μg/mL Refer to calcium standard conditions.
potassium as ionization suppressant. Prepare calibration standards containing 0,
For 0.04% Ba, the solution concentration will 20, 25, 30 μg/mL Ca. Each solution must
be approximately 2 μg/mL Ba. contain 2000 μg/mL potassium.
Standard Preparation
Kyanite
Refer to barium standard conditions.
Al (Aluminium)
Prepare calibration standards containing 0, 1,
2, 3 μg/mL Ba. The standard solutions must Range
contain the same reagents and major matrix
15-25% Al
elements as the sample solutions at
approximately the same concentration. For Typical Analysis
example, in the typical case above the
standards would contain: Al 24% Si 22% Fe 0.1%
For 0.5% Hg, the solution concentration will Prepare standards containing 200, 600,
be approximately 50 μg/mL Hg. 1000 μg/mL B.
Standard Preparation
Si (Silicon)
Refer to mercury standard conditions.
Typical Analysis
Prepare calibration standards containing 0,
Refer to boron in borax ore.
25, 50, 100 μg/mL Hg. The standard solutions
must contain the same reagents and major Sample Preparation
matrix elements as the sample solutions at
approximately the same concentration. For Refer to boron in borax ore.
example, in the typical case above the For 2% Si, the solution concentration will be
standards would contain: approximately 200 μg/mL Si.
2.5% tartaric acid Standard Preparation
5% hydrochloric acid Refer to silicon standard conditions.
Prepare calibration standards containing 0, For example, in the typical case above the
25, 50, 75 μg/mL Zr. The standard solutions standards would contain:
must contain the same reagents and major
Pb 450 μg/mL
matrix elements as the sample solutions at
approximately the same concentration. For Zn 700 μg/mL
example, in the typical case above the
standards would contain: HCl (1:1) 5 mL/10 mL
Zn (Zinc)
WARNING Corrosive Liquid and Toxic Hazard
Range
Bromine (liquid/vapor) is highly
corrosive and toxic. Take suitable 6.5–15.0% Zn
precautions when handling this Sample Preparation
chemical or else a serious injury
could result. Refer to copper in sulfide ores.
Take 2 mL of prepared solution and add 5 mL
of 1:1 hydrochloric acid. Dilute to 100 mL
with 10% w/v ammonium acetate. For 6.7% Zn
the dilute solution will contain approximately
Aqua regia (hydrochloric/nitric acid; 3:1): 14 μg/mL Zn.
Prepare 100 mL of aqua regia by mixing
75 mL concentrated hydrochloric acid with Standard Preparation
25 mL concentrated nitric acid. Refer to zinc standard conditions.
Tartaric acid solution (10% w/v): Prepare calibration standards containing 0,
Dissolve 10 g A.R. tartaric acid in 100 mL 10, 20, 30 μg/mL Zn. The standard solutions
distilled water. must contain the same reagents and major
Sample Preparation matrix elements as the sample solutions at
approximately the same concentration.
Dry a portion of finely ground sample at
110°C. Weigh 0.500 g dried sample into a For example, in the typical case above, the
covered beaker and add 10 mL bromine- standards would contain:
carbon tetrachloride mixture. Allow to stand HCl (1:1) 5 mL/100 mL
for 10 minutes with periodic swirling. Add
10 mL aqua regia and allow to stand for a ammonium acetate 10% w/v
further 10 minutes. With the beaker still
covered, heat gently on a water bath to drive Tin Ores
off excess bromine (1–1.5 hour). Do not
evaporate to dryness. Add 20 mL tartaric acid Sn (Tin)
solution (10% w/v) and heat for a further
2 minutes. Cool, transfer to a 100 mL Range
volumetric flask and make up to volume with Suitable for levels near 0.1%.
distilled water.
Typical Analysis
For analysis, add 10 mL of prepared solution
to 10 mL of hydrochloric acid and dilute to Sn 0.15% WO3 0.2%
100 mL.
SiO2 remainder
For 15.5% Sb, the analytical solution will
Interferences
contain approximately 78 μg/mL Sb.
At 224.6 nm, non-atomic species may absorb
Standard Preparation
even in the nitrous oxide-acetylene flame. Use
Refer to antimony standard conditions. a background corrector to check for the
presence of non-atomic absorption.
Prepare calibration standards containing 0,
50, 75, 100 μg/mL Sb. Sample Preparation
The standard solutions must contain the same Fuse 1.000 g sample and 5 g sodium peroxide
reagents and major elements as the sample in a zirconium crucible at dull red heat until a
solutions at approximately the same clear melt is obtained.
concentration. For example, in the typical
case above the standards would contain:
hydrochloric acid 10 mL/100 mL
tartaric acid (10% w/v) 2 mL/100 mL
W (Tungsten)
Typical Analysis
Refer to tin in tin ores.
Interferences
SiO2 is separated and standard additions are
used to compensate for Ca interference.
Sample Preparation
Add 50 mL hydrochloric acid to 1.000 g
samples and heat at 70 °C for 3 hours. Allow
to stand overnight and evaporate down to
10 mL to remove excess acid. Cool and dilute
to 100 mL. For 0.2% WO3 in a 1.000 g sample,
this is 16 μg/mL W in solution. A 20 mL
aliquot contains approximately 320 μg W.
Standard Preparation
Refer tungsten standard conditions.
Stock 1000 μg/mL solution is required.
Sample Preparation Fe 1%
At this concentration the other interferences
Weigh 2.000 g of sample into a PTFE beaker,
are suppressed.
add 5 mL of nitric acid and warm slowly. Add
5 mL of hydrochloric acid dropwise with
constant stirring until the reaction subsides. Iron Alloy
Heat to near boiling for half an hour and cool.
Add 2 mL of hydrofluoric acid very slowly so Al (Aluminium)
that the temperature of the mix does not
Typical Analysis
exceed 35–40 °C, and let stand for half an
hour to dissolve silicon, titanium and Al 0.005% Mn 0.75%
vanadium.
Cr 0.04% Si 0.03%
Filter the solution to remove carbon. Ash the
filter and the residue in a platinum crucible. Cu 0.02% Fe remainder
Rinse the crucible with a few drops of Interferences
hydrofluoric and hydrochloric acids and add
to the filtrate. The large excess of iron in the matrix causes
interference effects in the determination of
Dilute to 200 mL in a plastic volumetric flask. each of the trace elements. This is minimized
Dilute 10 mL of this solution to 100 mL. by the use of standards which contain a
similar amount of iron to that in the sample.
For 1% Cu, the final solution concentration
will be approximately 10 μg/mL. In the total trace element analysis of a
complex sample, an alternative to employing
Standard Preparation individual element standards is to prepare a
range of composite standards which have a
Refer to copper standard conditions.
base of the major matrix element. The same
Prepare calibration standards containing 0, 5, range of standards is then employed in all
10, 15 μg/mL Cu. The standard solutions must trace metal determinations in the parent
contain the same reagents and major matrix sample. An example of this is given in the
elements as the sample solutions at determination of Al, Cr, Cu, Mn, Si in iron
approximately the same concentration. For alloy.
example, in the typical case above the
Aluminium is partially ionized in the nitrous
standards would contain:
oxide-acetylene flame. To suppress ionization,
Fe 900 μg/mL add potassium nitrate or chloride to give a
final concentration of 1000 μg/mL potassium
Ti (Titanium) in all sample and standard solutions,
including the blank.
Typical Analysis
Refer to copper in carbon steels.
Sample Preparation
Refer to copper in carbon steels; use the
undiluted sample solution which contains
approximately 10 μg/mL Ti.
Cr (Chromium)
Sample Preparation
Typical Analysis
Take 0.5 g catchweight samples in PTFE
Refer to aluminium in iron alloy. beakers. Add 20 mL nitric acid and 10 mL
hydrochloric acid and warm slowly. When the
Interferences reaction subsides, heat to near boiling for
A range of composite standards, prepared in 30 minutes, then cool. Add 10 mL
a pure iron matrix, is used to compensate for hydrofluoric acid, keeping the temperature
the large excess of iron in the sample. below 50 °C to avoid loss of silicon. Allow to
Chemical interference by the iron is overcome stand for 5 minutes, then add 0.5 g boric acid
by the use of a nitrous oxide-acetylene flame. to remove excess fluoride and dissolve any
precipitated iron fluorides. Dilute to 100 mL,
Sample Preparation then further dilute 2 mL to 100 mL for
potassium determination. For 0.09% K in a
Refer to aluminium in iron alloy.
0.5 g sample, the final solution concentration
For 0.04% Cr, the sample solution will be approximately 1 μg/mL K.
concentration will be approximately 8 μg/mL
Standard Preparation
Cr.
Refer to potassium standard conditions.
Standard Preparation
Prepare calibration standards of 0, 0.5, 1.0,
Refer to aluminium in iron alloy.
1.5 μg/mL K, each containing 600 μg/mL iron
The composite standards will contain 0, 3, 7, to approximate the sample solution matrix.
10 μg/mL Cr.
Mn (Manganese)
Cu (Copper)
Typical Analysis
Typical Analysis
Refer to aluminium in iron alloy.
Refer to aluminium in iron alloy.
Interferences
Interferences
A range of composite standards, prepared in
A range of composite standards, prepared in a pure iron matrix, is used to compensate for
a pure iron matrix, is used to compensate for the large excess of iron in the sample.
the large excess of iron in the sample.
Sample Preparation
Sample Preparation
Refer to aluminium in iron alloy.
Refer to aluminium in iron alloy.
For 0.75% Mn, the sample solution
For 0.02% Cu, the sample solution concentration will be approximately
concentration will be approximately 4 μg/mL 150 μg/mL Mn.
Cu.
Standard Preparation
Standard Preparation
Refer to aluminium in iron alloy.
Refer to aluminium in iron alloy.
The composite standards will contain 0, 100,
The composite standards will contain 0, 2, 4, 150, 200 μg/mL Mn.
6 μg/mL Cu.
Si (Silicon)
K (Potassium)
Typical Analysis
Typical Analysis
Refer to aluminium in iron alloy.
Fe 63% Ti 1.2% Si 3%
Interferences
K 0.09% Al 1.4% Na 0.17%
A range of composite standards, prepared in
a pure iron matrix, is used to compensate for
the large excess of iron in the sample.
Mg (Magnesium) Al (Aluminium)
Range Range
0.001–0.25% Mg 2–4% Al
Interferences Typical Analysis
In the air-acetylene flame, aluminium Fe 83% Si 1.4% Ca 0.52%
depresses the Mg absorbance by 17–20% at
Mg 0.36% Ti 1.2% V 0.6%
the levels encountered in iron and steel.
Mn 0.08% Al 3% Na 0.17%
This and other minor interferences can be
overcome by the addition of 1500 μg/mL Remainder: Cr, Ni, etc.
strontium to the sample solutions.
Interferences
The method is satisfactory in the presence of
the following elements: Silicon suppresses the aluminium absorbance
by up to 30%. This is overcome by using
Ni 30% Cr 30% Cu 10% Mo 5% standards containing silicon at the same
concentration as the sample.
Mn 2% Si 2% Al 2% V 2%
Aluminium is partially ionized in the nitrous
P 2% Zn 1% Ti 0.5% Pb 0.5%
oxide-acetylene flame. To suppress ionization,
Interferences are minimized without the need add potassium nitrate or chloride solution to
for a suppressor when the nitrous oxide- give a final concentration of 2000 μg/mL
acetylene flame is used. potassium in all solutions including the blank.
Reference Sample Preparation
Australian Standard K1, Part 20 (1964). Dissolve 0.500 g sample in 20 mL nitric acid,
10 mL hydrochloric acid in a PTFE beaker.
Sample Preparation
Heat to aid dissolution.
Dissolve 1.000 g of sample in 30 mL Cool; add 10 mL hydrofluoric acid slowly so
hydrochloric acid (1:1) and oxidize with 5 mL
that the temperature of the beaker is
nitric acid. Evaporate to dryness and bake for
maintained at 50–60 °C to prevent
5 minutes at 200 °C. Extract the residue with
volatilization of the silicon.
10 mL hydrochloric acid; heat for 5 minutes
to ensure dissolution of the soluble salts. Add 0.5 g A.R. boric acid to complex excess
Dilute with 50 mL cold water and cool. Add hydrofluoric acid; add 0.2 g potassium as the
5 mL strontium solution (183 g/litre nitrate and dilute to 100 mL.
SrCl2.2H2O) and dilute to 200 mL in a
For 3% Al, the solution concentration will be
graduated flask. Filter off a portion,
approximately 150 μg/mL Al.
discarding the first washings.
Notes:
Standard Preparation
If silicon, titanium and niobium are not
Refer to magnesium standard conditions.
present in the sample, the hydrofluoric
Prepare calibration standards of a acid treatment may be omitted.
concentration range designed to cover the
Use the method of standard additions to
expected magnesium level in the sample
correct for the complex matrix of the
solution.
sample solutions.
The standard solutions must contain all
Standard Preparation
reagents and major elements present in the
sample solution at approximately the Refer to aluminium standard conditions.
concentration of the sample.
Refer to aluminium in steels. For 1.2% Ti, the solution concentration will be
approximately 60 μg/mL Ti.
Sample Preparation
Standard Preparation
Refer to aluminium in steels. For 0.08% Mn
the solution concentration will be 4 μg/mL Refer titanium standard conditions.
Mn. Only the 1000 μg/mL stock solution is
Standard Preparation required; the standard addition method is
used to avoid matching samples and
Refer to manganese standard conditions. standards.
Only the 1000 μg/mL Mn standard solution is
required. The standard addition procedure is V (Vanadium)
used to avoid matching the complicated Typical Analysis
solution matrix.
Refer to aluminium in steels.
Na (Sodium) Interferences
Typical Analysis Many elements present will interfere. Use the
Refer to aluminium in steels. method of standard additions to compensate
for the interferences.
Sample Preparation
Sample Preparation
Refer to aluminium in steels. For 0.17% Na in
a 0.500 g sample the solution concentration Refer to aluminium in steels.
will be 8.5 μg/mL. Standard Preparation
Standard Preparation Refer to vanadium standard conditions.
Refer to sodium standard conditions. An aqueous solution only is required as the
Dilute the 1000 μg/mL standard solution to method of standard additions is used.
100 μg/mL. The standard addition method is
used so that matrix matching is unnecessary. Stainless Steel
Si (Silicon) Cr (Chromium)
Typical Analysis Typical Analysis
Refer to aluminium in steels. Cr 15% Nb 1% Si 0.5%
Sample Preparation Mn 2% Ni 8% Ta 0.04%
Refer to aluminium in steels. Mo 0.03% Fe remainder
Standard Preparation Interferences
Refer to silicon standard conditions. A nitrous oxide-acetylene flame is used to
overcome chemical interference from iron
Prepare standards containing 0, 20, 40 μg/mL
and nickel.
added Si by pipetting 0, 1, 2 mL aliquots of a
1000 μg/mL Si standard into 25 mL aliquots 50% (v/v) ethanol is added to improve
of sample solution. Dilute to 50 mL. sensitivity.
For 8% Ni, the dilute solution will contain Prepare calibration standards containing 0,
approximately 40 μg/mL Ni. 100, 150, 200, 250 μg/mL Nb. The standard
solutions must contain the same reagents and
Standard Preparation
major matrix elements as the sample
Refer to nickel standard solutions. solutions at approximately the same
concentration. For example, in the typical
Prepare calibration standards containing 0, case above the standards would contain:
10, 30, 50 μg/mL Ni. The standard solutions
must contain the same reagents and major HCl 5%
matrix elements as the sample solutions at HF 2%
approximately the same concentration.
Ethanol 50%
For example, in the typical case above the
standards would contain: NH4F 10 mL/100 mL of 1 M solution
Fe 500 μg/mL Fe 2.5 g/100 mL
Cr 75 μg/mL
Ta (Tantalum)
hydrochloric acid 2 mL/100 mL
Typical Analysis
ethanol 50 mL/100 mL
Refer to chromium in stainless steel.
Nb (Niobium) Interferences
Typical Analysis Ammonium fluoride and ethanol are used to
improve the sensitivity and minimize
Refer to chromium in stainless steel.
interferences.
Interferences Sample Preparation
Many of the elements present interfere. Add
Refer to niobium in stainless steel.
ammonium fluoride and ethanol to the
solution to increase the niobium absorbance For 0.04% Ta, the solution concentration will
and suppress the interferences. be approximately 10 μg/mL Ta.
References Standard Preparation
1. Headridge, J.B. and Hubbard, D.P., Anal. Refer tantalum standard conditions.
Chim. Acta., 37, 151 (1967).
Prepare calibration standards containing 0, 5,
2. Bond, A.M., Anal. Chem., 42, 932 (1970). 10, 15, 20 μg/mL Ta. The standard solutions
must contain the same reagents and major
Sample Preparation
matrix elements as the sample solutions at
Dissolve 2.5 g samples in 10 mL hydrochloric approximately the same concentration. For
acid, with careful dropwise addition of 3 mL example, in the typical case above the
nitric acid and 2 mL hydrofluoric acid in a standards would contain:
PTFE beaker. Evaporate to moist salts.
Dissolve the salts in 5 mL hydrochloric acid,
2 mL hydrofluoric acid and 5 mL water. Add
10 mL 1 M ammonium fluoride and 50 mL
ethanol, and dilute to 100 mL in a plastic
volumetric flask. For 1% Nb the solution
concentration will be 250 μg/mL.
Standard Preparation
Refer to niobium standard conditions.
hydrochloric acid 20 mL/100 mL Use the dilute solution; for 13.2% Si, the
solution concentration will be approximately
nitric acid 4 mL/100 mL 70 μg/mL Si.
hydrofluoric acid 4 mL/100 mL Standard Preparation
boric acid 0.5 g/100 mL Refer to silicon standard conditions.
Prepare calibration standards containing 0,
Pb (Lead)
50, 75, 100 μg/mL Si. The standard solutions
Typical Analysis must contain the same reagents and major
matrix elements as the sample solutions at
Refer to aluminium in aluminium-silicon approximately the same concentration. For
alloy. example, in the typical case above the
standards would contain:
Ni (Nickel) HCl 5%
Sample Preparation
Niobium Alloy
Refer to bismuth in nickel alloys.
Nb (Niobium)
For 0.0025% Pb, the solution concentration
will be approximately 1 μg/mL Pb. Typical Analysis
Standard Preparation Nb 52%
Refer to lead standard conditions. Sample Preparation
Prepare calibration standards containing 0, 1, Dissolve 0.200 g samples in 10 mL
2, 3 μg/mL Pb. hydrofluoric acid and 3 mL nitric acid in a
PTFE beaker. Evaporate to dryness, cool and
The standard solutions must contain the same
dissolve the solids in 4 mL hydrofluoric acid
reagents and major matrix elements as the and 3 mL nitric acid. Dilute to 100 mL in a
sample solutions at approximately the same plastic volumetric flask. For 52% Nb in a
concentration. For example, in the typical 0.200 g sample, the solution concentration
case above the standards would contain: will be approximately 1000 μg/mL Nb.
Ni 22000 μg/mL HCl 8 mL/100 mL Standard Preparation
Cr 4000 μg/mL HNO3 4 mL/100 mL
Refer to niobium standard conditions.
Al 2000 μg/mL HF 2 mL/100 mL
Prepare calibration standards containing 0,
Ti 2000 μg/mL Boric acid solution 500, 1000, 1500 μg/mL Nb. The standard
0.1% solutions must contain the same reagents and
major matrix elements as the sample
Si (Silicon) solutions at approximately the same
concentration. For example, in the typical
Typical Analysis case above the standards would contain:
Si 0.5% HF 4%
Sample Preparation HNO3 3%
Refer to chromium in nickel alloy. Ti 1000 μg/mL
For 0.5% Si, the solution concentration will be
approximately 50 μg/mL Si. Ti (Titanium)
Pb (Lead)
Range
0.002–0.006% Pb
Interferences
A range of composite standards, prepared in
a pure zinc matrix, is used to compensate for
the large excess of zinc in the sample.
At the 217.0 nm wavelength, non-atomic
species in the air-acetylene flame absorb
strongly. Use a background corrector to check
for the presence of non-atomic absorption.
Sample Preparation
Refer to aluminium in zinc alloy.
Use the undiluted solution; for 0.003% Pb, the
solution concentration will be approximately
0.3 μg/mL Pb.
Standard Preparation
Refer to aluminium in zinc alloy.
The composite standards will contain 0, 0.2,
0.3, 0.4, 0.6 μg/mL Pb.
Standard Preparation
Refer to selenium standard conditions.
Prepare calibration standards containing 0,
0.005, 0.01, 0.02, 0.04, 0.06, 0.08, 0.1 μg/mL
(mg/L) selenium so that 10 mL aliquots will
contain 0, 50, 100, 200, 400, 600, 800, 1000 ng
selenium.
Sewage Effluent
Cr (Chromium)
Range
0.1–1.0 μg/mL Cr
Interferences
High levels of iron, cobalt and chloride can
cause interference unless optimum flame
conditions are used.
Sample Preparation
Samples must be collected in acid washed
containers. Acidify the sample by addition of
hydrochloric acid to level of 1%.
Standard Preparation
Refer to chromium standard conditions.
Prepare calibration standards containing 0,
0.1, 0.5 and 1.0 μg/mL Cr in 1% hydrochloric
acid.